Water-soluble fluorine-containing modified N-NVP polymer and preparation method thereof

Abstract

The invention relates to a water-soluble fluorine-containing modified N-NVP polymer and a preparation method thereof. The preparation method comprises the step: N-NVP and DFMA are subjected to a polymeric reaction to obtain the compound shown as the formula (I). According to the invention, as a fluorine-containing hydrophobic alkyl side chain is introduced to the water-soluble N-NVP polymer, the N-NVP polymer has the advantages of excellent hydrophobic association property, high surface activity, and excellent salt, temperature and shear resistant properties, can serve as a macromolecular surfactant, and meanwhile has a high utilization potentiality in the fields of oil exploitation, paints, medicines, daily chemicals and the like.

Description

technical field

[0001] The invention relates to a water-soluble polymer containing fluorine-modified N-vinylpyrrolidone and a preparation method thereof, in particular to a water-soluble polyN-vinylpyrrolidone (NVP) / dodecafluoroheptyl methacrylate (DFMA) A polymer and a preparation method thereof belong to the technical field of water-soluble polymer synthesis. Background technique

[0002] Since polyvinylpyrrolidone and vinylpyrrolidone copolymers have many excellent physical and chemical properties, such as excellent solubility, low toxicity, film-forming properties, solubilization, complexation, physiological compatibility, surface activity and chemical stability etc. Therefore, it is widely used in medical and health care, cosmetics, food, beverage, brewing, papermaking, textile printing and dyeing, new materials, suspension and emulsion polymerization, dispersion stability and other fields, and has attracted more and more attention from scientific researchers.

[0003] ...

Examples

Embodiment 1

[0051] A preparation method of a water-soluble polymer containing fluorine-modified N-vinylpyrrolidone, the steps are as follows:

[0052] (1) Weigh 8.3g (0.07477mol) of N-vinylpyrrolidone (NVP) monomer, and measure 50mL of toluene, add it into a 100mL three-necked flask equipped with a nitrogen tube, a condenser tube and a stirring bar, and stir until completely dissolved;

[0053] (2) Weigh 0.09 g (0.225 mmol) of dodecafluoroheptyl methacrylate (DFMA), add it into a three-neck flask, fill it with nitrogen gas at room temperature, and fully stir until dissolved;

[0054] (3) Weigh 0.0839 g of azobisisobutyronitrile, add it to a three-neck flask, put it in a constant temperature water bath at 25°C, and blow nitrogen gas for 0.5 h;

[0055] (4) Raise the reaction temperature to 85°C and react for 8 hours to obtain a water-soluble polymer containing fluorine-modified N-vinylpyrrolidone.

[0056] Subsequent treatment: the water-soluble polymer of fluorine-modified N-vinylpyrrolid...

Embodiment 2

[0060] As described in Example 1, the difference is that the amount of N-vinylpyrrolidone monomer in step (1) is 11.1 g;

[0061] The feeding amount of monomer dodecafluoroheptyl methacrylate (DFMA) in step (2) is 0.2 g.

[0062] 10.012 g of water-soluble polymer powder containing fluorine-modified N-vinylpyrrolidone was obtained, and the yield was ≥88%. Molecular weight M w =(2.291±0.609)×10 5 g·mol -1 .

[0063] The water-soluble polymer containing fluorine-modified N-vinylpyrrolidone prepared in this example has high surface activity at room temperature, the concentration of its aqueous solution is 10 mg / mL, and the surface tension of the aqueous solution can be reduced to 33 mN / m.

Embodiment 3

[0065] As described in Example 1, the difference is that the amount of N-vinylpyrrolidone monomer in step (1) is 7.87g;

[0066] The feeding amount of monomer dodecafluoroheptyl methacrylate (DFMA) in step (2) is 0.2 g.

[0067] 6.983 g of water-soluble polymer powder containing fluorine-modified N-vinylpyrrolidone was obtained, and the yield was ≥86%. Molecular weight M w =(2.380±0.426)×10 5 g·mol -1 .

[0068] The water-soluble polymer containing fluorine-modified N-vinylpyrrolidone prepared in this example has high surface activity at room temperature, the concentration of its aqueous solution is 10 mg / mL, and the surface tension of the aqueous solution can be reduced to 33 mN / m.

technical field

[0001] The invention relates to a water-soluble polymer containing fluorine-modified N-vinylpyrrolidone and a preparation method thereof, in particular to a water-soluble polyN-vinylpyrrolidone (NVP) / dodecafluoroheptyl methacrylate (DFMA) A polymer and a preparation method thereof belong to the technical field of water-soluble polymer synthesis. Background technique

[0002] Since polyvinylpyrrolidone and vinylpyrrolidone copolymers have many excellent physical and chemical properties, such as excellent solubility, low toxicity, film-forming properties, solubilization, complexation, physiological compatibility, surface activity and chemical stability etc. Therefore, it is widely used in medical and health care, cosmetics, food, beverage, brewing, papermaking, textile printing and dyeing, new materials, suspension and emulsion polymerization, dispersion stability and other fields, and has attracted more and more attention from scientific researchers.

[0003] ...

Examples

Embodiment 1

[0051] A preparation method of a water-soluble polymer containing fluorine-modified N-vinylpyrrolidone, the steps are as follows:

[0052] (1) Weigh 8.3g (0.07477mol) of N-vinylpyrrolidone (NVP) monomer, and measure 50mL of toluene, add it into a 100mL three-necked flask equipped with a nitrogen tube, a condenser tube and a stirring bar, and stir until completely dissolved;

[0053] (2) Weigh 0.09 g (0.225 mmol) of dodecafluoroheptyl methacrylate (DFMA), add it into a three-neck flask, fill it with nitrogen gas at room temperature, and fully stir until dissolved;

[0054] (3) Weigh 0.0839 g of azobisisobutyronitrile, add it to a three-neck flask, put it in a constant temperature water bath at 25°C, and blow nitrogen gas for 0.5 h;

[0055] (4) Raise the reaction temperature to 85°C and react for 8 hours to obtain a water-soluble polymer containing fluorine-modified N-vinylpyrrolidone.

[0056] Subsequent treatment: the water-soluble polymer of fluorine-modified N-vinylpyrrolid...

Embodiment 2

[0060] As described in Example 1, the difference is that the amount of N-vinylpyrrolidone monomer in step (1) is 11.1 g;

[0061] The feeding amount of monomer dodecafluoroheptyl methacrylate (DFMA) in step (2) is 0.2 g.

[0062] 10.012 g of water-soluble polymer powder containing fluorine-modified N-vinylpyrrolidone was obtained, and the yield was ≥88%. Molecular weight M w =(2.291±0.609)×10 5 g·mol -1 .

[0063] The water-soluble polymer containing fluorine-modified N-vinylpyrrolidone prepared in this example has high surface activity at room temperature, the concentration of its aqueous solution is 10 mg / mL, and the surface tension of the aqueous solution can be reduced to 33 mN / m.

Embodiment 3

[0065] As described in Example 1, the difference is that the amount of N-vinylpyrrolidone monomer in step (1) is 7.87g;

[0066] The feeding amount of monomer dodecafluoroheptyl methacrylate (DFMA) in step (2) is 0.2 g.

[0067] 6.983 g of water-soluble polymer powder containing fluorine-modified N-vinylpyrrolidone was obtained, and the yield was ≥86%. Molecular weight M w =(2.380±0.426)×10 5 g·mol -1 .

[0068] The water-soluble polymer containing fluorine-modified N-vinylpyrrolidone prepared in this example has high surface activity at room temperature, the concentration of its aqueous solution is 10 mg / mL, and the surface tension of the aqueous solution can be reduced to 33 mN / m.

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